CN107464963B - A method of efficiently separating valuable material from waste lithium cell - Google Patents
A method of efficiently separating valuable material from waste lithium cell Download PDFInfo
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- CN107464963B CN107464963B CN201710626490.XA CN201710626490A CN107464963B CN 107464963 B CN107464963 B CN 107464963B CN 201710626490 A CN201710626490 A CN 201710626490A CN 107464963 B CN107464963 B CN 107464963B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
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Abstract
The present invention discloses a kind of method that valuable material is efficiently separated from waste lithium cell comprising step: waste lithium cell being classified according to model difference, discharge treatment is carried out in discharge equipment, dismantling obtains internal battery core and outsourcing aluminum hull；Battery core impregnates filtering oil removing through the broken organic solvent that is added；Add water and stir simultaneously settle and separate diaphragm；Filter powder is through wet ball-milling and is diluted with water carry out flotation, isolates high purity graphite, aluminium powder；Change pulp density and flotation conditions carry out secondary flotation, flotation upper layer positive mix, flotation lower layer copper powder can be obtained.Separation method of the present invention is simple, low energy consumption, environmental pollution is small, production intensity is low, and each valuable material is efficiently separated in old and useless battery, good separating effect, the high feature of the rate of recovery, has preferable productivity effect.
Description
Technical field
It is specifically a kind of that valuable material is efficiently separated from waste lithium cell the present invention relates to waste lithium cell recycling field
Method.
Background technique
The recyclable part of waste and old lithium ion battery mainly includes positive electrode, negative electrode material, electrolyte, diaphragm, shell, cover board
Deng.Its anode is generally with lithium base inlaid scheme LixMyXz(M common is nickel, cobalt, manganese, vanadium, iron etc.), PVDF, aluminium foil are main base
Raw material；Negative electrode material generally comprises graphite, adhesive and copper foil etc.；Electrolyte is usually with LiPF6Based on conductive salt, with
Mixed solvent system based on EC, PC, DMC, EMC；Diaphragm is generally polyethylene, microporous polypropylene membrane and propylene and ethylene
Copolymer, Natene etc.；Shell is generally aluminum material；Cover board generally comprises positive and negative anodes lappet, washer, top layer
Deng.Since lithium battery type is more, established rules lattice, material, size, electrical property difference are larger when producing, but due to its electrification
Learn that mechanism is similar, and manufacturing process, raw material, auxiliary material are close, it is different only doping metals, solvent burden ratio, substance filling with
And different from various modifying agent, this provides possibility to efficiently separate each valuable material from waste lithium cell.
As the application of lithium battery obtains development at full speed, the separation and recovery of rear valuable material is scrapped, will be become important
The technical issues of.Waste lithium cell is separated and is handled, current most of domestic and international patents and manufacturer all use
Roasting direct after simple dismantling makes organic matter volatilization or high-temperature decomposition reaction occurs, and such method can generate a large amount of toxic
Pernicious gas, simultaneously because the presence of hydrogen fluoride, is proposed high requirement to subsequent air flue equipment and treatment process.How will
The valuable materials such as waste lithium cell outsourcing aluminum hull, cover board, organic matter reagent, diaphragm, positive mix, cathode graphite, copper foil, aluminium foil
It is efficiently separated, its subsequent technique will be produced bigger effect.
Summary of the invention
It is an object of the invention to overcome defect of the existing technology, one kind is provided and is efficiently separated from waste lithium cell
The method of valuable material.
The purpose of the present invention can be achieved through the following technical solutions:
A method of efficiently separating valuable material from waste lithium cell, specifically includes the following steps:
(1) physics discharges: waste lithium cell being classified according to model difference, is carried out at electric discharge in discharge equipment
Reason, until voltage reduces to 0.5V or less；
(2) it disassembles: to the lithium battery that discharged obtained by step (1), being cut under sealing and circulating flow conditions, cut surface
In cover board 1~3cm backward, internal battery core and outsourcing aluminum hull are obtained after dismantling；
(3) closed broken: to battery core obtained by step (2), break process to be carried out under sealing and circulating flow conditions, when being crushed
Between 2~10min, 5~20mm of particle size after cracking, dismantling with it is broken when spillage enter overflow launder, volatile organic matter cooling gaseous fluid
Change, is collected；
(4) it impregnates dissolution: by particle obtained by step (3), organic solvent is added and carries out immersion treatment, positive mix, cathode
Graphite is able to fall off from pole plate, and filtering obtains 1# mixed powder；The control of organic solvent additional amount is in solid-to-liquid ratio in waste lithium cell
1:0.5~3,15~40 DEG C of soaking temperature, 1~2h of soaking time；
(5) it stands membrane removal: by 1# mixed powder obtained by step (4), adding water and stirring and stand, filter to obtain 2# mixed powder；
(6) wet ball-milling: by 2# mixed powder obtained by step (5), being fitted into ball mill and ground, enter abrasive grain≤
20mm, abrasive concentration 25~50%, 20~50r/min of mill speed, 0.5~1h of abrasive material time, out abrasive grain degree≤0.25mm；
(7) by ball milling powder obtained by step (6) by pulp density 10~20% plus water, pH adjusting agent control 1# flotation: is added
Bubble 10~20min of time, regulator A dosage, are scraped in slurry pH=6~7 by 20~40 DEG C of slurry temperature, 3~10min of inflationtime
It is smart twice to carry out roughing three times by 5000~8000g/t, collecting agent A 100~800g/t of dosage, 50~200g/t of frother dosages
The flotation mode of choosing, makes ball milling powder isolate high purity graphite, aluminium powder, obtains 3# mixed powder；
(8) by 3# mixed powder obtained by step (7) by pulp density 10~15% plus water, pH adjusting agent control 2# flotation: is added
Bubble 8~10min of time, is scraped in slurry pH=5~6.5 processed by 25~40 DEG C of slurry temperature, 5~10min of inflationtime, and regulator B is used
8000~10000g/t, collecting agent B 200~300g/t of dosage, 300~500g/t of frother dosages are measured, roughing one twice is carried out
Secondary selected flotation mode, isolates positive mix and copper powder.
Further scheme, -20~50 DEG C of discharge equipment operating temperature in the step (1), discharge voltage adjustable range 0~
220V。
Further scheme, the step (2) and sealing and circulating air-flow in (3) are nitrogen, in argon gas, helium, carbon dioxide
One or more mixing.
Further scheme, organic solvent is styrene, tetrachloro-ethylene, trichloro ethylene, ethylene glycol in the step (4)
One of ether, acetone, isopropanol, ethylene glycol monobutyl ether or a variety of mixing.
Further scheme, ball mill is horizontal tank abrading-ball grinding machine, conical ball mill or tubular type ball milling in the step (6)
Machine；Mill ball material used in ball mill is 201 stainless steels, 304 stainless steels or corundum.
Further scheme, pH adjusting agent is sulfuric acid, hydrochloric acid, nitric acid, acetic acid, one in phosphoric acid in the step (7) and (8)
Kind or a variety of mixing.
Further scheme, the step (7) and foaming agent in (8) are turpentine oil, 2# flotation oil, cresotinic acid, weigh in pyridine
One or more mixing.
Further scheme, regulator A is one or two kinds of mixing of starch, waterglass in the step (7)；Collecting agent A
For one of kerosene, diesel oil, xanthate, two acetic acid of cetyl or a variety of mixing.
Further scheme, regulator B is one of lime, starch, waterglass, tannin, vulcanized sodium in the step (8)
Or a variety of mixing；Collecting agent B is one of kerosene, light diesel, two acetic acid of cetyl or a variety of mixing.
Compared with prior art, beneficial effects of the present invention: waste lithium cell valuable material is separated step by step, technique
Process is simple, equipment requirement is low, has abandoned and roasts this committed step to waste lithium cell in the prior art, avoids exhaust gas dirt
Dye and loss of material；It is disassembled and is crushed under sealing and circulating air flow system, solved in waste lithium cell removal process
The secondary pollution problem of organic matter and inorganic salts；Each valuable material rate of recovery is good, separation purity is high, battery core contained by waste lithium cell
And aluminum hull, the rate of recovery is up to 99.8%, and the organic matter rate of recovery is up to 95%, and for the diaphragm rate of recovery up to 98%, recycling graphite rate is reachable
98%(purity 99.5%), aluminium powder and the copper powder rate of recovery are up to 99%(purity 98%), the positive mix rate of recovery is up to 97.8%.
Detailed description of the invention
Fig. 1 is a kind of flow chart for the method that valuable material is efficiently separated from waste lithium cell of the present invention.
Specific embodiment
In order to illustrate more clearly of the purpose of the present invention, advantage, technical solution, process route, below with reference to embodiment and
Attached drawing, the present invention is described in further detail, and exemplary embodiment of the invention and its explanation are only used for explaining this hair
It is bright, it is not as a limitation of the invention.
Embodiment 1
Waste lithium cell is classified according to model difference, in lithium battery discharge equipment, waste lithium cell is carried out
Electric quantity test, and it is greater than the lithium battery external load of 0.5V to voltage, it is connected by battery with resistance, using exothermic process to disappear
The electricity in power consumption pond makes its single battery voltage reduce to 0.5V or less；Under the conditions of sealing and circulating nitrogen atmosphere, cut
And dismantling, cut surface obtain internal battery core and outsourcing aluminum hull at the 3cm of cover board end after dismantling, the rate of recovery is up to 99.8%, battery core
By closed broken, being crushed average particle size is 20mm, and spillage enters overflow launder when disassembling and is broken, and volatile organic matter gas is cold
But liquefy, tetrachloro-ethylene is added by solid-to-liquid ratio 1:3 in particle, impregnate 2h under the conditions of 15 DEG C, positive mix, cathode graphite be able to from
It falls off on pole plate, organic reagent is dissolved in organic phase and is separated, the 1# mixed powder after oil removing, by solid-to-liquid ratio 1:2
It adding water and stirring and stands, be directly separated on the diaphragm floating water surface, electrolyte lithium salt, lithium based additive are reacted with water in refuse battery,
Water phase containing lithium is formed, by filtering, reaches separation of solid and liquid；2# mixed powder is put into XMQ-67 type conical ball mill, and abrasive material is dense
25%, drum's speed of rotation 20r/min are spent, 30min is ground, discharging wet screening is crossed 60 meshes, is diluted with water, and pulp density is controlled
10%, addition salt acid for adjusting pH=6,40 DEG C of slurry temperature, kerosene 800g/t, 2# flotation oil mass 50g/t, starch 5000g/t, three times
Roughing inflation 3min, scrape bubble 8min, obtain the graphite (purity 99.7%) of the rate of recovery 98.1%, twice selected inflation 5min, scrape bubble
20min obtains the aluminium powder (purity 98.1%) of the rate of recovery 99.3%；The gained 3# mixed powder after 1# flotation, adjustment slurry are dense
Degree 15%, addition salt acid for adjusting pH=5.0,25 DEG C of slurry temperature, light diesel 300g/t, 2# flotation oil mass 300g/t, starch
Inflation 5min, 8000g/t, lime 2000g/t scrape bubble 8min, flotation upper layer obtains the positive mix rate of recovery 97.8%, and lower layer is
Copper powder, rate of recovery 99%(purity 98.4%).
Embodiment 2
By waste lithium cell (model: 18650), in lithium battery discharge equipment, to waste lithium cell carry out electric quantity test,
And it is greater than the lithium battery external load of 0.5V to voltage, it is connected by battery with resistance, using exothermic process to consume battery
Electricity makes its voltage reduce to 0.5V hereinafter, being cut and being disassembled, cut surface exists under the conditions of sealing and circulating helium atmosphere
At the 1cm of cover board end, internal battery core and outsourcing aluminum hull are obtained after dismantling, for battery core by closed broken, being crushed average particle size is 5mm,
Styrene is added by solid-to-liquid ratio 1:0.5 in particle, 1h is impregnated under the conditions of 40 DEG C, positive mix, cathode graphite are able to from pole plate
It falls off, organic reagent is dissolved in organic phase and is separated, and the 1# mixed powder after oil removing adds water to stir by solid-to-liquid ratio 1:2
It mixes and stands, be directly separated on the diaphragm floating water surface, electrolyte lithium salt, lithium based additive are reacted with water in refuse battery, and formation contains
Lithium water phase reaches separation of solid and liquid by filtering；2# mixed powder is put into horizontal tank abrading-ball grinding machine, abrasive concentration 50%, ball milling
Machine revolving speed 50r/min grinds 1h, and discharging wet screening is crossed 60 meshes, is diluted with water, and controls pulp density 20%, sulfuric acid tune is added
Save pH=7,20 DEG C of slurry temperature, diesel oil 100 g/t, 2#Inflation 5min, flotation oil mass 200g/t, waterglass 8000g/t scrape bubble
10min, obtains the graphite (purity 99.6%) of the rate of recovery 98.5%, and the aluminium powder (purity 98.4%) of the rate of recovery 99.1% is floating by 1#
Gained 3# mixed powder after choosing, adjustment pulp density 20%, addition sulphur acid for adjusting pH=6.5,40 DEG C of slurry temperature, kerosene 50g/t,
Light diesel 200g/t, 2#Inflation 10min, flotation oil mass 500 g/t, starch 10000g/t scrape bubble 10min, flotation upper layer obtains
To the positive mix rate of recovery 97.4%, lower layer is copper powder, rate of recovery 99.3%(purity 98.7%).
Embodiment 3
Waste lithium cell (model: 20100140), in lithium battery discharge equipment, is subjected to electricity survey to waste lithium cell
Examination, and it is greater than the lithium battery external load of 0.5V to voltage, it is connected by battery with resistance, using exothermic process to consume battery
Electricity, so that its voltage is reduced to 0.5V hereinafter, being cut and being disassembled under the conditions of sealing and circulating nitrogen atmosphere, cut surface
At the 2cm of cover board end, internal battery core and outsourcing aluminum hull are obtained after dismantling, by closed broken, broken average particle size is battery core
Styrene is added by solid-to-liquid ratio 1:3 in 20mm, particle, and 1.5h is impregnated under the conditions of 30 DEG C, and organic reagent is dissolved in organic phase and obtains
With separation, 1# mixed powder after oil removing is added water and stirred and is stood by solid-to-liquid ratio 1:2, is directly divided on the diaphragm floating water surface
From electrolyte lithium salt, lithium based additive are reacted with water in refuse battery, form water phase containing lithium, by filtering, reach separation of solid and liquid；
2# mixed powder is put into XMQ-67 type conical ball mill, abrasive concentration 30%, drum's speed of rotation 50r/min, grinds 1h, discharging
Wet screening crosses 60 meshes, is diluted with water, control pulp density 20%, addition phosphorus acid for adjusting pH=6.8, and 30 DEG C of slurry temperature, coal
Oil 150 g/t, 2#Inflation 5min, flotation oil mass 200g/t, starch 6000g/t scrape bubble 10min, obtain the stone of the rate of recovery 98.5%
Black (purity 99.5%), the aluminium powder (purity 98.4%) of the rate of recovery 99.1%, the gained 3# mixed powder after 1# flotation, adjustment material
Slurry concentration 10%, addition phosphorus acid for adjusting pH=6.2,40 DEG C of slurry temperature, light diesel 50g/t, turpentine oil mass 450g/t, solvable shallow lake
Inflation 5min, powder 8500g/t scrapes bubble 10min, flotation upper layer obtains the positive mix rate of recovery 97.8%, and lower layer is copper powder, recycling
Rate 99%(purity 98.1%).
Claims (9)
1. a kind of method for efficiently separating valuable material from waste lithium cell, which is characterized in that specifically includes the following steps:
(1) physics discharges: waste lithium cell is classified according to model difference, discharge treatment is carried out in discharge equipment, until
Voltage reduces to 0.5V or less；
(2) it disassembles: to the lithium battery that discharged obtained by step (1), being cut under sealing and circulating flow conditions, cut surface is covering
Plate 1~3cm backward, obtains internal battery core and outsourcing aluminum hull after dismantling；
(3) closed broken: to battery core obtained by step (2), break process is carried out under sealing and circulating flow conditions, is crushed the time 2
~10min, 5~20mm of particle size after cracking, spillage enters overflow launder when disassembling and is broken, and volatile organic matter gas cooling liquefies,
It is collected；
(4) it impregnates dissolution: by particle obtained by step (3), organic solvent is added and carries out immersion treatment, positive mix, cathode graphite
It is able to fall off from pole plate, filters, obtain 1# mixed powder；The control of organic solvent additional amount is in solid-to-liquid ratio 1 in waste lithium cell:
0.5~3,15~40 DEG C of soaking temperature, 1~2h of soaking time；
(5) it stands membrane removal: by 1# mixed powder obtained by step (4), adding water and stirring and stand, filter to obtain 2# mixed powder；
(6) wet ball-milling: by 2# mixed powder obtained by step (5), being fitted into ball mill and ground, enter abrasive grain≤
20mm, abrasive concentration 25~50%, 20~50r/min of mill speed, 0.5~1h of abrasive material time, out abrasive grain degree≤0.25mm；
(7) 1# flotation: by ball milling powder obtained by step (6) by pulp density 10~20% plus water, pH adjusting agent is added and controls slurry
PH=6~7, scrape and steep 10~20min of time by 20~40 DEG C of slurry temperature, 3~10min of inflationtime, and regulator A dosage 5000~
8000g/t, collecting agent A 100~800g/t of dosage, 50~200g/t of frother dosages carry out selected twice floating of roughing three times
Mode is selected, ball milling powder is made to isolate high purity graphite, aluminium powder, obtains 3# mixed powder；
(8) by 3# mixed powder obtained by step (7) by pulp density 10~15% plus water, pH adjusting agent control material 2# flotation: is added
PH=5~6.5 are starched, 25~40 DEG C of slurry temperature, 5~10min of inflationtime, scrape bubble 8~10min of time, regulator B dosage
It is primary to carry out roughing twice by 8000~10000g/t, collecting agent B 200~300g/t of dosage, 300~500g/t of frother dosages
Selected flotation mode, isolates positive mix and copper powder.
2. a kind of method for efficiently separating valuable material from waste lithium cell according to claim 1, which is characterized in that
- 20~50 DEG C of discharge equipment operating temperature in the step (1), 0~220V of discharge voltage adjustable range.
3. a kind of method for efficiently separating valuable material from waste lithium cell according to claim 1, which is characterized in that
The step (2) and sealing and circulating air-flow in (3) are one of nitrogen, argon gas, helium, carbon dioxide or a variety of mix.
4. a kind of method for efficiently separating valuable material from waste lithium cell according to claim 1, which is characterized in that
Organic solvent is styrene, tetrachloro-ethylene, trichloro ethylene, ethylene glycol ether, acetone, isopropanol, second two in the step (4)
One of alcohol monobutyl ether or a variety of mixing.
5. a kind of method for efficiently separating valuable material from waste lithium cell according to claim 1, which is characterized in that
Ball mill is horizontal tank abrading-ball grinding machine, conical ball mill or tube mill in the step (6)；Mill ball material used in ball mill
Matter is 201 stainless steels, 304 stainless steels or corundum.
6. a kind of method for efficiently separating valuable material from waste lithium cell according to claim 1, which is characterized in that
The step (7) and pH adjusting agent in (8) are one of sulfuric acid, hydrochloric acid, nitric acid, acetic acid, phosphoric acid or a variety of mix.
7. a kind of method for efficiently separating valuable material from waste lithium cell according to claim 1, which is characterized in that
The step (7) and foaming agent in (8) are one of turpentine oil, 2# flotation oil, cresotinic acid, weight pyridine or a variety of mix.
8. a kind of method for efficiently separating valuable material from waste lithium cell according to claim 1, which is characterized in that
Regulator A is one or two kinds of mixing of starch, waterglass in the step (7)；Collecting agent A is kerosene, diesel oil, xanthate, ten
One of six alkyl, two acetic acid or a variety of mixing.
9. a kind of method for efficiently separating valuable material from waste lithium cell according to claim 1, which is characterized in that
Regulator B is one of lime, starch, waterglass, tannin, vulcanized sodium or a variety of mixing in the step (8)；Collecting agent B
For one of kerosene, light diesel, two acetic acid of cetyl or a variety of mixing.
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| CN108550940A (en) * | 2018-04-25 | 2018-09-18 | 河南师范大学 | The resource utilization reuse method of waste and old lithium ion battery lithium iron phosphate positive material |
| CN108767353B (en) * | 2018-05-25 | 2020-08-04 | 北京矿冶科技集团有限公司 | Method for producing lithium-rich clean liquid from anode active material of waste lithium ion battery |
| CN109713394B (en) * | 2019-01-18 | 2021-08-06 | 中国矿业大学 | Method for separating lithium cobaltate and graphite in waste electrode material |
| CN110564978A (en) * | 2019-10-15 | 2019-12-13 | 俞杰 | operation process for recovering nickel and cobalt in ternary battery material by wet method |
| CN111484008B (en) * | 2020-04-16 | 2021-12-07 | 中国恩菲工程技术有限公司 | Composite regulator for graphite flotation in waste lithium ion batteries and recovery method of graphite in waste lithium ion batteries |
| CN113560308A (en) * | 2020-04-29 | 2021-10-29 | 南通江海储能技术有限公司 | Method for separating current collector and active material of capacitor and positive and negative active materials |
| EP4107810A4 (en) * | 2020-06-08 | 2024-03-20 | Ascend Elements Inc | Anode recovery in recycled batteries |
| CN112157107A (en) * | 2020-08-28 | 2021-01-01 | 威立雅新能源科技(江门)有限公司 | Method for separating positive and negative electrode materials from waste lithium batteries |
| CN112670614B (en) * | 2020-12-29 | 2022-11-22 | 广东省科学院资源综合利用研究所 | Physical sorting method for positive and negative electrode materials of waste lithium iron phosphate batteries |
| CN113502396A (en) * | 2021-05-31 | 2021-10-15 | 广东邦普循环科技有限公司 | Method for safely leaching waste battery and application |
| CN114665225B (en) * | 2022-04-18 | 2023-12-01 | 四川卓勤新材料科技有限公司 | Automatic oil filtering system of lithium ion battery diaphragm production line and control method |
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